#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/70/1517066.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1517066
loop_
_publ_author_name
'Tiffany M. Smith'
'Diona Symester'
'Kathryn Perrin'
'Jose Vargas'
'Michael Tichenor'
'Charles J. O-Connor'
'Jon Zubieta'
_publ_section_title
;
 Hydrothermal syntheses and structural chemistry of Mn(II), Co(II) and
 Ni(II) coordination polymers with xylyl-diphosphonate ligands
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              46
_journal_page_last               59
_journal_volume                  402
_journal_year                    2013
_chemical_formula_moiety         'C20 H18 Co N2 O6 P2'
_chemical_formula_sum            'C20 H18 Co N2 O6 P2'
_chemical_formula_weight         503.23
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 98.0770(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.099(2)
_cell_length_b                   12.0022(12)
_cell_length_c                   7.5739(8)
_cell_measurement_reflns_used    3920
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      28.06
_cell_measurement_theta_min      3.24
_cell_volume                     1898.9(3)
_computing_cell_refinement       'Bruker SAINT (Bruker, 2011)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2011)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2011)'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2010)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2011)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0189
_diffrn_reflns_av_sigmaI/netI    0.0174
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            7687
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    1.118
_exptl_absorpt_correction_T_max  0.9159
_exptl_absorpt_correction_T_min  0.8965
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS SHELXL-97 (Sheldrick, 2008)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.760
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1028
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.422
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         1940
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0250
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0372P)²+3.5871P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0659
_refine_ls_wR_factor_ref         0.0681
_reflns_number_gt                1815
_reflns_number_total             1940
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-402-46-59-9.cif
_cod_data_source_block           compound_9
_cod_original_cell_volume        1899.0(3)
_cod_original_sg_symbol_Hall     -C2yc
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               1517066
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Co1 Co 0.5000 0.34475(3) 0.2500 0.00866(11) Uani 1 2 d S
P1 P 0.41489(2) 0.57324(4) 0.07309(5) 0.00937(12) Uani 1 1 d .
O1 O 0.43492(6) 0.65125(10) -0.06346(16) 0.0122(3) Uani 1 1 d .
O2 O 0.42494(6) 0.63360(10) 0.25908(16) 0.0142(3) Uani 1 1 d .
H2' H 0.4339 0.5874 0.3384 0.017 Uiso 1 1 calc R
O3 O 0.44413(6) 0.45754(10) 0.08274(15) 0.0116(3) Uani 1 1 d .
N1 N 0.44407(7) 0.20432(12) 0.14030(18) 0.0112(3) Uani 1 1 d .
C1 C 0.47137(10) -0.10113(15) 0.1965(2) 0.0192(4) Uani 1 1 d .
H1 H 0.4521 -0.1685 0.1599 0.023 Uiso 1 1 calc R
C2 C 0.44026(9) 0.00151(15) 0.1392(2) 0.0160(4) Uani 1 1 d .
C3 C 0.38021(9) 0.00625(16) 0.0301(2) 0.0193(4) Uani 1 1 d .
H3 H 0.3587 -0.0590 -0.0074 0.023 Uiso 1 1 calc R
C4 C 0.35407(9) 0.10750(17) -0.0197(2) 0.0181(4) Uani 1 1 d .
H4 H 0.3144 0.1117 -0.0907 0.022 Uiso 1 1 calc R
C5 C 0.38748(8) 0.20511(16) 0.0373(2) 0.0139(4) Uani 1 1 d .
H5 H 0.3693 0.2734 0.0014 0.017 Uiso 1 1 calc R
C6 C 0.46965(8) 0.10378(14) 0.1923(2) 0.0122(3) Uani 1 1 d .
C7 C 0.32904(8) 0.54969(15) 0.0229(2) 0.0130(3) Uani 1 1 d .
H7A H 0.3205 0.5105 -0.0899 0.016 Uiso 1 1 calc R
H7B H 0.3161 0.5013 0.1141 0.016 Uiso 1 1 calc R
C8 C 0.28812(8) 0.65278(15) 0.0118(2) 0.0129(4) Uani 1 1 d .
C9 C 0.25229(9) 0.68091(16) 0.1468(2) 0.0151(4) Uani 1 1 d .
H9 H 0.2535 0.6349 0.2460 0.018 Uiso 1 1 calc R
C10 C 0.28514(8) 0.72354(15) -0.1354(2) 0.0150(4) Uani 1 1 d .
H10 H 0.3085 0.7064 -0.2271 0.018 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O3 Co1 O3 99.69(7) 2_655 .
O3 Co1 O1 86.80(5) 2_655 6_566
O3 Co1 O1 91.51(5) . 6_566
O3 Co1 O1 91.51(5) 2_655 5_665
O3 Co1 O1 86.80(5) . 5_665
O1 Co1 O1 177.38(7) 6_566 5_665
O3 Co1 N1 165.28(5) 2_655 .
O3 Co1 N1 92.35(5) . .
O1 Co1 N1 84.44(5) 6_566 .
O1 Co1 N1 97.62(5) 5_665 .
O3 Co1 N1 92.35(5) 2_655 2_655
O3 Co1 N1 165.28(5) . 2_655
O1 Co1 N1 97.62(5) 6_566 2_655
O1 Co1 N1 84.44(5) 5_665 2_655
N1 Co1 N1 77.15(8) . 2_655
O1 P1 O3 116.91(7) . .
O1 P1 O2 108.35(7) . .
O3 P1 O2 112.08(7) . .
O1 P1 C7 108.77(8) . .
O3 P1 C7 104.72(8) . .
O2 P1 C7 105.29(8) . .
P1 O1 Co1 138.69(7) . 5_665
P1 O2 H2' 109.5 . .
P1 O3 Co1 144.04(7) . .
C5 N1 C6 117.62(15) . .
C5 N1 Co1 128.13(12) . .
C6 N1 Co1 114.17(11) . .
C1 C1 C2 120.80(11) 2_655 .
C1 C1 H1 119.6 2_655 .
C2 C1 H1 119.6 . .
C6 C2 C3 117.05(17) . .
C6 C2 C1 119.85(18) . .
C3 C2 C1 123.11(17) . .
C4 C3 C2 119.43(17) . .
C4 C3 H3 120.3 . .
C2 C3 H3 120.3 . .
C3 C4 C5 119.47(17) . .
C3 C4 H4 120.3 . .
C5 C4 H4 120.3 . .
N1 C5 C4 122.99(17) . .
N1 C5 H5 118.5 . .
C4 C5 H5 118.5 . .
N1 C6 C2 123.42(16) . .
N1 C6 C6 117.24(10) . 2_655
C2 C6 C6 119.34(11) . 2_655
C8 C7 P1 115.50(12) . .
C8 C7 H7A 108.4 . .
P1 C7 H7A 108.4 . .
C8 C7 H7B 108.4 . .
P1 C7 H7B 108.4 . .
H7A C7 H7B 107.5 . .
C10 C8 C9 118.01(16) . .
C10 C8 C7 120.43(16) . .
C9 C8 C7 121.56(16) . .
C10 C9 C8 121.10(17) 7_565 .
C10 C9 H9 119.5 7_565 .
C8 C9 H9 119.5 . .
C9 C10 C8 120.89(16) 7_565 .
C9 C10 H10 119.6 7_565 .
C8 C10 H10 119.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O3 2.0994(12) 2_655
Co1 O3 2.0994(12) .
Co1 O1 2.1046(12) 6_566
Co1 O1 2.1046(12) 5_665
Co1 N1 2.1559(15) .
Co1 N1 2.1559(15) 2_655
P1 O1 1.4992(12) .
P1 O3 1.5172(13) .
P1 O2 1.5717(12) .
P1 C7 1.8199(17) .
O1 Co1 2.1046(12) 5_665
O2 H2' 0.8200 .
N1 C5 1.332(2) .
N1 C6 1.357(2) .
C1 C1 1.357(4) 2_655
C1 C2 1.434(3) .
C1 H1 0.9300 .
C2 C6 1.408(3) .
C2 C3 1.413(3) .
C3 C4 1.366(3) .
C3 H3 0.9300 .
C4 C5 1.404(3) .
C4 H4 0.9300 .
C5 H5 0.9300 .
C6 C6 1.445(4) 2_655
C7 C8 1.504(2) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C8 C10 1.396(2) .
C8 C9 1.396(2) .
C9 C10 1.388(3) 7_565
C9 H9 0.9300 .
C10 C9 1.388(3) 7_565
C10 H10 0.9300 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O3 P1 O1 Co1 -5.34(15) . 5_665
O2 P1 O1 Co1 122.43(11) . 5_665
C7 P1 O1 Co1 -123.60(12) . 5_665
O1 P1 O3 Co1 120.25(12) . .
O2 P1 O3 Co1 -5.69(15) . .
C7 P1 O3 Co1 -119.32(13) . .
O3 Co1 O3 P1 -28.80(10) 2_655 .
O1 Co1 O3 P1 58.21(13) 6_566 .
O1 Co1 O3 P1 -119.78(13) 5_665 .
N1 Co1 O3 P1 142.71(12) . .
N1 Co1 O3 P1 -173.30(15) 2_655 .
O3 Co1 N1 C5 131.76(19) 2_655 .
O3 Co1 N1 C5 -13.29(14) . .
O1 Co1 N1 C5 78.00(14) 6_566 .
O1 Co1 N1 C5 -100.38(14) 5_665 .
N1 Co1 N1 C5 177.14(17) 2_655 .
O3 Co1 N1 C6 -44.8(3) 2_655 .
O3 Co1 N1 C6 170.13(11) . .
O1 Co1 N1 C6 -98.58(11) 6_566 .
O1 Co1 N1 C6 83.05(11) 5_665 .
N1 Co1 N1 C6 0.56(8) 2_655 .
C1 C1 C2 C6 0.8(3) 2_655 .
C1 C1 C2 C3 -179.0(2) 2_655 .
C6 C2 C3 C4 0.7(3) . .
C1 C2 C3 C4 -179.51(17) . .
C2 C3 C4 C5 0.4(3) . .
C6 N1 C5 C4 -0.5(2) . .
Co1 N1 C5 C4 -176.93(12) . .
C3 C4 C5 N1 -0.6(3) . .
C5 N1 C6 C2 1.7(2) . .
Co1 N1 C6 C2 178.66(13) . .
C5 N1 C6 C6 -178.53(17) . 2_655
Co1 N1 C6 C6 -1.6(2) . 2_655
C3 C2 C6 N1 -1.8(3) . .
C1 C2 C6 N1 178.37(16) . .
C3 C2 C6 C6 178.42(18) . 2_655
C1 C2 C6 C6 -1.4(3) . 2_655
O1 P1 C7 C8 -56.17(14) . .
O3 P1 C7 C8 178.13(12) . .
O2 P1 C7 C8 59.78(14) . .
P1 C7 C8 C10 74.04(19) . .
P1 C7 C8 C9 -105.83(17) . .
C10 C8 C9 C10 -0.1(3) . 7_565
C7 C8 C9 C10 179.77(16) . 7_565
C9 C8 C10 C9 0.1(3) . 7_565
C7 C8 C10 C9 -179.77(16) . 7_565
